US20190368016A1 - Steel suitable for plastic moulding tools - Google Patents
Steel suitable for plastic moulding tools Download PDFInfo
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- US20190368016A1 US20190368016A1 US16/310,185 US201716310185A US2019368016A1 US 20190368016 A1 US20190368016 A1 US 20190368016A1 US 201716310185 A US201716310185 A US 201716310185A US 2019368016 A1 US2019368016 A1 US 2019368016A1
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- powder
- steel
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 69
- 239000010959 steel Substances 0.000 title claims abstract description 69
- 238000010137 moulding (plastic) Methods 0.000 title abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 50
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims description 34
- 229910001566 austenite Inorganic materials 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 25
- 229910000859 α-Fe Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 229910000734 martensite Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000007373 indentation Methods 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 238000009689 gas atomisation Methods 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 7
- 239000004033 plastic Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 230000003749 cleanliness Effects 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 238000007751 thermal spraying Methods 0.000 claims description 4
- 238000001513 hot isostatic pressing Methods 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 238000010288 cold spraying Methods 0.000 claims description 2
- 238000004372 laser cladding Methods 0.000 claims description 2
- 238000009704 powder extrusion Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 239000002344 surface layer Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 23
- 239000000956 alloy Substances 0.000 abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 26
- 239000011651 chromium Substances 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 17
- 239000011572 manganese Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000010949 copper Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 230000032683 aging Effects 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 8
- 150000004767 nitrides Chemical class 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 6
- 229910052748 manganese Inorganic materials 0.000 description 6
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 description 6
- 238000004881 precipitation hardening Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000010955 niobium Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 230000000717 retained effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910000943 NiAl Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- -1 aluminium nitrides Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001887 electron backscatter diffraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B22F1/0014—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/115—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by spraying molten metal, i.e. spray sintering, spray casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
- B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the invention relates to a steel.
- the invention relates to precipitation hardening steel suitable for the manufacturing of plastic moulding tools.
- Precipitation hardening stainless steels embrace 17-7 PH, 17-4 PH, 15-5 PH, PH 15-7Mo, PH 14-8Mo and PH 13-8Mo.
- the latter steel is also designated 1.4534, X3CrNiMoAl13-8-2 and 513800.
- the chemical composition of PH 13-8 Mo is (in wt. %): C: ⁇ 0.05, Si: ⁇ 0.1, Mn: ⁇ 0.1, P: ⁇ 0.01, S: ⁇ 0.008, Cr: 12.25-13.25, Ni: 7.5-8.5, Mo: 2.0-2.5, N: ⁇ 0.01, Ti: ⁇ 0.1, Al: 0.8-1.35, balance Fe.
- a steel of this type is known as Böhler N709.
- EP 459 547 discloses a precipitation hardenable stainless steel intended for plastic forming moulds, wherein the nitrogen content is restricted as much as possible in order to avoid the formation of hard nitrides, which impair the polishability.
- Steels of this type are commonly used for parts requiring a high strength and a good toughness. Typical applications of these steels are aircraft parts, springs and plastics moulds.
- steels are often delivered in a solution treated condition and are hardenable by aging to a hardness in the range of 34-52 HRC.
- Important properties are a high strength and corrosion resistance as well as a good polishability.
- plastic mould steels should also have a good machinability and good welding properties such that the steels can be welded without preheating and postheating.
- This invention is directed to an alternative composition to an alloy of the type PH 13-8Mo.
- the object of the present invention is to provide a steel having an improved property profile and being suitable for plastic moulding.
- the present invention aims at providing a precipitation hardening mould steel having a high strength and toughness as well as a high cleanliness, a good polishability and uniform properties also in large dimensions.
- the invention aims at providing the steel in form of powder, in particular but not restricted to steel powder suitable for Additive Manufacturing (AM).
- AM Additive Manufacturing
- a further object is to provide a steel, which can be used to obtain articles having a prolonged life.
- the general object is solved by providing a steel consisting of, in weight % (wt. %):
- the steel fulfils at least one of the following requirements:
- the steel has a mean hardness in the range of 320-510 HBW 10/3000 , wherein the steel has a thickness of at least 100 mm and the maximum deviation from the mean Brinell hardness value in the thickness direction measured in accordance with ASTM E10-01 is less than 10%, preferably less than 7%, less than 5%, less than 3% or even less than 1%, and wherein the minimum distance of the centre of the indentation from the edge of the specimen or edge of another indentation shall be at least two and a half times the diameter of the indentation and the maximum distance shall be no more than 4 times the diameter of the indentation, and/or the steel has a cleanliness fulfilling the following maximum requirements with respect to micro-slag according to ASTM E45-97, Method A:
- the steel has a cleanliness fulfilling the following maximum requirements:
- the steel may be alloyed with S in order to improve the machinability. However, it need not be alloyed with S, in particular when produced by Powder Metallurgy (PM).
- the steel composition may then fulfil at least one of the following requirements:
- microstructure may fulfil at least one of the following requirements:
- the steel alloy can be provided in the form of a pre-alloyed powder having a composition as shown above.
- the pre-alloyed powder can be produced by gas atomizing. It is preferred that at least 80% of the powder particles have a size in the range of 5 to 150 ⁇ m so that the powder fulfils at least one of the following requirements:
- the powder particles have a size in the range of 10 to 100 ⁇ m and that the powder fulfils at least one of the following requirements:
- Powder size distribution (in ⁇ m): 10 ⁇ D10 ⁇ 30 25 ⁇ D50 ⁇ 45 D90 ⁇ 70 Mean sphericity, SPHT ⁇ 0.90 Mean aspect ratio, b/l ⁇ 0.88
- the pre-alloyed described above can be used to form an article by the use of an additive manufacturing method.
- the article may fulfil at least one of the following requirements:
- the article is at least a part of a mould for forming plastic and the said article may optionally fulfil at least one of the following requirements:
- the invention is also directed to the use of the inventive pre-alloyed powder for making a solid object by the use of any of the methods of hot isostatic pressing, powder extrusion and additive manufacturing or for providing a surface layer on a substrate by thermal spraying, laser cladding, cold spraying or overlay welding.
- Carbon is effective for improving the strength and the hardness of the steel. However, if the content is too high, the steel may be difficult to machine after cooling from hot working. C should be present in a minimum content of 0.02%, preferably at least 0.025%. The upper limit for carbon is 0.04%, preferably 0.035%. The nominal content is 0.030%.
- Silicon is used for deoxidation. Si is also a strong ferrite former. Si is therefore limited to 0.45%.
- the upper limit may be 0.40, 0.35, 0.34, 0.33, 0.32, 0.31, 0.30, 0.29 or 0.28%.
- the lower limit may be 0.12, 0.14, 0.16, 0.18 or 0.20%. Preferred ranges are 0.15-0.40% and 0.20-0.35%.
- Manganese contributes to improving the hardenability of the steel. If the content is too low then the hardenability may be too low. At higher sulphur contents manganese prevents red brittleness in the steel. Manganese shall therefore be present in a minimum content of 0.10%, preferably at least 0.15, 0.20, 0.25 or 0.30%.
- the steel shall contain maximum 0.5% Mn, preferably maximum 0.45, 0.40 or 0.35%. A preferred range is 020-0.40%.
- Chromium is to be present in a content of at least 11% in order to make the steel stainless and to provide a good hardenability in larger cross sections during the heat treatment.
- high amounts of Cr may lead to the formation of high-temperature ferrite, which reduces the hot-workability.
- the lower limit may be 11.2, 11.4, 11.6 or 11.8%.
- the upper limit Cr is 13% and the amount of Cr may be limited or 12.8, 12.6, 12.4 or 12.2%.
- a preferred range is 11.5-12.5%.
- Nickel is an austenite stabilizer, which and suppresses the formation of delta ferrite. Nickel gives the steel a good hardenability and toughness. Nickel is also beneficial for the machinability and polishability of the steel. Nickel is essential for the precipitation hardening as it together with Al form minute intermetallic NiAl-particles during aging. However, excess Ni additions may result in too high an amount of retained austenite.
- the lower limit may therefore be 7.2, 7.4, 7.6, 7.8, 8.0, 8.2, 8.4, 8.6, 8.8, 9.0 or 9.1%.
- the upper limit may be 10.0, 9.8, 9.6 or 9.4%. A preferred range is 8.5-10 or 9.0-9.5%.
- the total content of Cr and Ni is 19-23%.
- the lower amount may be 19.5, 20.0, 20.5 20.6, 20.7, 20.8 or 20.9%.
- the upper limit may be 22.8, 22.7, 22.6, 22.5, 22.4, 22.3, 22.2, 22.1, 22.0, 21.9, 21.8, 21.7, 21.6, 21.5, 21.4 or 21.3%
- a preferred range is 20.5-22.0%, preferably 20.5-22.0, most preferably 20.8-21.7%.
- Mo in solid solution is known to have a very favourable effect on the hardenability.
- Molybdenum is a strong carbide forming element and also a strong ferrite former.
- a controlled amount of Mo in the matrix counteracts the formation of reverted austenite during aging. For this reason the amount of Mo should be 1-2%.
- the lower limit may be 1.1, 1.2, 1.3 or 1.4%.
- the upper limit may be 1.9, 1.8, 1.7, 1.6, or 1.5%.
- Molybdenum can also be used in higher amounts in combination with Boron in order to obtain a desired amount of hard borides of the type M 2 M′B 2 , where M and M′ stand for metals.
- M is Mo
- M′ is Fe
- the boride may contain minor amounts of other elements such as Cr and Ni.
- Mo 2 FeB 2 will simply be referred to as Mo 2 FeB 2 .
- the maximum content of molybdenum is therefore 25%.
- the contents of Mo and B should be balanced such that the content of Mo in solid solution in the matrix remains in the range of 1-2%.
- Aluminium is used for precipitation hardening in combination with Ni.
- the upper limit is restricted to 2.0% in order to avoid the formation of too much delta ferrite.
- the upper limit may be 1.95, 1.90, 1.85, 1.80 or 1.75%.
- the lower limit may be 1.45, 1.50, 1.55, 1.60 or 1.65%.
- Nitrogen is a strong austenite former and also a strong nitride former. N may be used in in an amount of up to 0.75% in Nitride Dispersion Strengthened (NDS) alloys. NDS alloys can be produced with basically the same techniques as ODS alloys.
- the nitrogen content may be restricted to 0.15%.
- the inventors of the present invention have surprisingly found, that nitrogen can be deliberately added to the steel without impairing the polishability, provided that the size of at least 80 vol. % of AlN particles present in the matrix is limited to not more than 4 ⁇ m. Preferably, the said size may restricted to 3 ⁇ m, 2 ⁇ m or even 1 ⁇ m. The small size of the nitrides also results in a grain refining effect.
- the lower limit for N may then be 0.011, 0.012, 0.013, 0.014, 0.015, 0.016, 0.017, 0.018, 0.019 or 0.02%.
- the upper limit may be 0.14, 0.12, 1.10, 0.08, 0.06, 0.05, 0.04 or 0.03%.
- the upper limit of nitrogen can be set to 0.040, 0.035, 0.030, 0.025 or 0.020%.
- Cu is an optional element, which may contribute to increase the hardness and the corrosion resistance of the steel.
- the ⁇ -Cu phase formed during aging not only reinforces the steel by precipitation hardening, but also affects the precipitation kinetics of the intermetallic phases. In addition thereto, it would appear that additions of Cu result in a slower growth of the intermetallic phase (NiAl) at higher working temperatures.
- the upper limit for Cu may be 2.3, 2.1, 1.9, 1.7, 1.5, 1.3, 1.1, 0.9, 0.7, 0.5, 0.3 or even 0.2%.
- the lower limit for Cu may 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 or 0.9%.
- the maximum allowable impurity content can be 0.2, 0.15 or 0.10%.
- Boron is an optional element that can be used in small amounts in order to increase the hardenability and to improve the hot workability of the stainless steel.
- the upper limit may then be set to 0.007, 0.006, 0.005 or 0.004%.
- B can also be used in higher amounts as a hard phase-forming element.
- B should then be at least 0.2% so as to provide the minimum amount of 3% hard phase Mo 2 FeB 2 .
- the amount of B is limited to 2.0% for not making the alloy too brittle.
- the lower limit may be set to 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 or 1.5%.
- the upper limit may be set to 1.4, 1.5, 1.6, 1.7, 1.8 or 1.9%.
- S may optionally be added in order to improve the machinability of the steel. If S is used for this purpose, then S is deliberately added to the steel in an amount of 0.01-0.25%. At higher sulphur contents there is a risk for red brittleness. Moreover, high sulphur contents may have a negative effect on the fatigue properties and on the polishability of the steel.
- the upper limit shall therefore be 0.25%, preferably 0.1% most preferably 0.03%.
- a preferred range is 0.015-0.030%.
- the amount of S is restricted to impurity contents as set out below.
- Nb is a strong carbide and nitride former. The content of this elements should therefore be limited in order to avoid the formation of undesired carbides and nitrides. The maximum amount of Nb is therefore 0.01%. Nb is preferably limited to 0.005%.
- These elements may form compounds with C, B, N and/or O. They can be used to produce an Oxide Dispersion Strengthened (ODS) or a Nitride Dispersion Strengthened (NDS) alloy.
- ODS Oxide Dispersion Strengthened
- NDS Nitride Dispersion Strengthened
- the upper limit is then 2% for each of these elements.
- the upper limit may be 1.5, 1.0, 0.5 or 0.3%. However, if these elements are not deliberately added for making an ODS alloy, then the upper limit may be 0.1, 0.05, 0.01 or 0.005%.
- the oxygen content is then preferably limited to 0.03%. However, if Oxygen is used in order to form an Oxide Dispersion Strengthened (ODS) alloy, then the upper limit may be as high as 0.80%.
- ODS Oxide Dispersion Strengthened
- the oxide can be admixed to a powder of be formed in-situ, e.g. by gas atomizing, in particular by using Gas Atomizing Reaction Synthesis (GARS) or during an Additive Manufacturing (AM) method, in particular through atmospheric reaction in Liquid Metal Deposition (LMD).
- GAS Gas Atomizing Reaction Synthesis
- AM Additive Manufacturing
- P, S and O are the main impurities, which may have a negative effect on the mechanical properties of the steel.
- P may therefore be limited to 0.05, 0.04, 0.03 0.02 or 0.01%.
- the impurity content of S may be limited to 0.05, 0.04, 0.003, 0.001, 0.0008, 0.0005 or even 0.0001%.
- the alloys of the present invention can be produced by any suitable method.
- suitable methods include:
- PM powders can be produced by conventional gas- or water-atomization of pre-alloyed steel.
- the powders can be used for thermal spraying, overlay welding, additive manufacturing (AM) or Metal Injection Moulding (MIM).
- AM additive manufacturing
- MIM Metal Injection Moulding
- gas-atomization is the preferred atomization method, because it is important to use a technique, that produces powder particles having a high degree of roundness and a low amount of satellites.
- the close-coupled gas atomization method can be used for this purpose.
- Powders produced by PM can be consolidated by Hot Isostatic Pressing (HIP) and/or by extrusion.
- the materials can be used as compacted or after subsequent hot working.
- the maximum size of the powder particles should normally be limited to 500 ⁇ m and, depending on the intended use, specific powder fractions may be used.
- the maximum size range is 5-150 ⁇ m, and the preferred size range is 10-100 ⁇ m with a mean size of about 25-45 ⁇ m.
- the preferred maximum size is 50 ⁇ m, for thermal spraying preferred ranges is 32-125 ⁇ m and 20-90 ⁇ m and for overlay welding the preferred range is 45-250 ⁇ m.
- the AM methods of prime interest are Liquid Metal Deposition (LMD), Selective Laser Melting (SLM) and Electron Beam (EB) melting.
- LMD Liquid Metal Deposition
- SLM Selective Laser Melting
- EB Electron Beam
- the powder characteristics are also of importance for AM.
- the powder size distribution measured with a Camsizer according to ISO 4497 should fulfil the following requirements (in ⁇ m):
- the powder should fulfil the following size requirements (in ⁇ m):
- the coarse size fraction D90 is limited to ⁇ 60 ⁇ m or even ⁇ 55 ⁇ m.
- the sphericity of the powder should be high.
- the mean SPHT should be at least 0.80 and can preferably be at least 0.85, 0.90, 0.91, 0.92 0.93, 0.94 or even 0.95.
- not more than 5% of the particles should have a SPHT ⁇ 0.70.
- Preferably said value should be less than 0.70, 0.65, 0.55 or even 0.50.
- the aspect ratio can be used in the classifying of the powder particles.
- the aspect ratio is defined as b/1, wherein b is the shortest width of the particle projection and 1 is the longest diameter.
- the mean aspect ratio should preferably be at least 0.85 or more preferably 0.86, 0.87, 0.88, 0.89, or 0.90.
- the inventive alloy is a precipitation hardenable steel having a martensitic matrix, which may comprise other microstructural constituents such as delta ferrite and austenite.
- the austenite may comprise retained and/or reverted austenite.
- the inventive alloy can be hardened by aging in the temperature range of 425-600° C. to a desired hardness in the range of about 34-56 HRC.
- the amount of delta ferrite should preferably be restricted to ⁇ 7 vol. %, preferably ⁇ 5 vol. %, more preferably ⁇ 3 vol. % for not impairing the hot workability.
- the austenite consists of retained and/or reverted austenite, in the following, austenite.
- Pre-alloyed powder produced by atomizing may contain substantial amounts of austenite but the amount of austenite in finished parts may be reduced to a lower level by solution heat treatment and/or ageing, if there is a fear that the austenite content is so high that it could lead to problems e.g. with respect to dimensional stability.
- the amount of austenite in the microstructure may therefore be limited to 22, 20, 18, 16, 14, 12, 10, 8, 6, 4 or 2 vol. %.
- austenite has a positive effect on the mechanical properties of the material, in particular the toughness, and is therefore a desired microstructural constituent in many applications.
- the inventive alloy can be hardened by aging in the temperature range of 425-600° C. to a desired hardness in the range of about 34-56 HRC.
- the alloy was produced in conventional way by induction melting, casting and forging.
- the alloy had the composition (in wt. %): C: 0.03, Si: 0.3, Mn: 0.2, Cr: 12.0, Ni: 9.3, Mo: 1.4, Al: 1.7, N: 0.017, balance Fe and impurities.
- the inventive alloy was compared to a commercial available steel of the type steel PH 13-8Mo (Böhler N709).
- the comparative alloy had the following nominal composition (in wt. %): C: 0.03, Si: ⁇ 0.08, Mn: ⁇ 0.08, Cr: 12.7, Ni: 8.1, Mo: 2.2, Al: 1.1, balance Fe.
- the inventive alloy differs from the comparative steel mainly in higher amounts of Mn, Si, Al and N and lower amounts of Mo dissolved in the matrix.
- the inventive steel and the comparative steel were both hardened to 50 HRC and subjected to un-notched impact testing using a standard specimen size of 10 mm ⁇ 10 mm ⁇ 55 mm.
- the inventive alloy was found to have an un-notched impact strength of 255 J, whereas the impact strength of the known steel was only 120 J.
- a base alloy having the composition similar to the alloy of Example 1 was produced in conventional way by induction melting, casting and forging.
- a ESR-remelted bar of the alloy was subjected to vacuum induction melting and closed couple gas atomization processing in order to obtain a powder suitable for AM processing.
- the gas to metal weight ratio during the atomization was 3:1.
- high purity (6N) nitrogen gas was used for the atomization.
- the particles obtained were examined with respect to size and shape by dynamic image processing according to ISO 13322-2.
- the powder was sieved in order to remove particles larger than 50 ⁇ m and smaller than 20 ⁇ m. The sieved powder was found to have the following size distribution: D10: 23 ⁇ m, D50: 34 ⁇ m and D90: 49 ⁇ m.
- the mean sphericity was 0.95 and the mean aspect ratio was 0.93.
- the powder had an oxygen content of 0.021% and a nitrogen content of 0.013%.
- the morphology of this powder was examined by Scanning Electron Microscopy (SEM and the powder was found to be almost fully spherical with a very low amount of satellites.
- the Apparent Density (AD) was 4.3 g/cm 3 and the Tap Density (TD) was 5.2 4.3 g/cm 3 .
- the powder produced would be expected to be suitable for AM processing.
- the as-built samples thus obtained had a density of 99.4% of the theoretical density (TD) and a hardness of 35 HRC at room temperature.
- the amount of austenite was about 23% in the sample.
- An examination in SEM using EBSD revealed that the austenite phase was extremely fine in size and dispersed at the boundaries of the martensite blocks.
- the influence of the thermal treatment of the built sample was examined. After ageing at 525° C. for 4 h the amount of austenite was reduced to 16 vol. %. However, an intermediate solution treatment at 850° C. for 30 minutes reduced the amount of austenite to 4 vol. %. The hardness of the solution annealed and aged sample was 50 HRC.
- the solution annealed and the aged sample have the same hardness as the conventionally produced sample of Example 1.
- the strength and elongation values were measured by uniaxial tensile testing and the impact toughness was measured by the Charpy V-notch test. The results are given below in Table 1. It can be seen that the material produced by AM has a considerably higher Impact toughness than the conventionally produced material and that the other mechanical values are comparable.
- the steel of the present invention is useful in large moulds or dies requiring a good corrosion resistance and a uniform hardness.
- the steel of the present invention is particular for making articles by AM.
Abstract
-
- C 0.02-0.04
- Si 0.1-0.4
- Mn 0.1-0.5
- Cr 11-13
- Ni 7-10
- Mo 1-25
- Al 1.4-2.0
- N 0.01-0.15
optional elements and impurities balance.
Description
- The invention relates to a steel. In particular, the invention relates to precipitation hardening steel suitable for the manufacturing of plastic moulding tools.
- Precipitation hardening stainless steels embrace 17-7 PH, 17-4 PH, 15-5 PH, PH 15-7Mo, PH 14-8Mo and PH 13-8Mo. The latter steel is also designated 1.4534, X3CrNiMoAl13-8-2 and 513800. The chemical composition of PH 13-8 Mo is (in wt. %): C: ≤0.05, Si: ≤0.1, Mn: ≤0.1, P: ≤0.01, S: ≤0.008, Cr: 12.25-13.25, Ni: 7.5-8.5, Mo: 2.0-2.5, N: ≤0.01, Ti: ≤0.1, Al: 0.8-1.35, balance Fe. A steel of this type is known as Böhler N709.
- EP 459 547 discloses a precipitation hardenable stainless steel intended for plastic forming moulds, wherein the nitrogen content is restricted as much as possible in order to avoid the formation of hard nitrides, which impair the polishability.
- Steels of this type are commonly used for parts requiring a high strength and a good toughness. Typical applications of these steels are aircraft parts, springs and plastics moulds.
- These steels are often delivered in a solution treated condition and are hardenable by aging to a hardness in the range of 34-52 HRC. Important properties are a high strength and corrosion resistance as well as a good polishability. In addition thereto, plastic mould steels should also have a good machinability and good welding properties such that the steels can be welded without preheating and postheating.
- This invention is directed to an alternative composition to an alloy of the type PH 13-8Mo.
- The object of the present invention is to provide a steel having an improved property profile and being suitable for plastic moulding. In particular the present invention aims at providing a precipitation hardening mould steel having a high strength and toughness as well as a high cleanliness, a good polishability and uniform properties also in large dimensions. In addition thereto, the invention aims at providing the steel in form of powder, in particular but not restricted to steel powder suitable for Additive Manufacturing (AM).
- A further object is to provide a steel, which can be used to obtain articles having a prolonged life.
- The foregoing objects, as well as additional advantages are achieved to a significant measure by providing a steel as defined in the alloy claims. A high and uniform hardness in combination with a high toughness result in a steel with good resistance to indentations and a minimum risk of unexpected failure, leading to a safer mould and a long tool life. The present inventors have found that it is possible to obtain a good polishability of the steel provided that the maximum size of the hard aluminium nitrides is controlled to be no larger than 4 μm.
- The invention is defined in the claims.
- The general object is solved by providing a steel consisting of, in weight % (wt. %):
-
Min Max C 0.02 0.04 Si 0.1 0.4 Mn 0.1 0.5 Cr 11 13 Ni 7 10 Cr + Ni 19 23 Mo 1 25 Al 1.4 2.0 N 0.01 0.75 optionally Cu 0.05 2.5 B 0.002 2.0 S 0.01 0.25 Nb 0.01 Ti 2 Zr 2 Ta 2 Hf 2 Y 2 Ca 0.0003 0.009 Mg 0.01 O 0.003 0.80 REM 0.2 Fe and impurities balance. - Preferably, the steel fulfils at least one of the following requirements:
-
Min Max C 0.025 0.035 Si 0.15 0.40 Mn 0.15 0.50 Cr 11.5 12.5 Ni 8.5 10.0 Cr + Ni 20 23 Mo 1.0 2.0 Al 1.5 1.9 N 0.01 0.15 S 0.01 0.03
and/or the steel has a mean hardness in the range of 320-510 HBW10/3000, wherein the steel has a thickness of at least 100 mm and the maximum deviation from the mean Brinell hardness value in the thickness direction measured in accordance with ASTM E10-01 is less than 10%, preferably less than 7%, less than 5%, less than 3% or even less than 1%, and wherein the minimum distance of the centre of the indentation from the edge of the specimen or edge of another indentation shall be at least two and a half times the diameter of the indentation and the maximum distance shall be no more than 4 times the diameter of the indentation, and/or
the steel has a cleanliness fulfilling the following maximum requirements with respect to micro-slag according to ASTM E45-97, Method A: -
A A B B C C D D T H T H T H T H 1.5 1.0 1.5 1.0 1.0 1.0 1.5 1.0 - Preferably, the steel has a cleanliness fulfilling the following maximum requirements:
-
A A B B C C D D T H T H T H T H 1.0 0 1.5 1.0 0 0 1.5 1.0 - The steel may be alloyed with S in order to improve the machinability. However, it need not be alloyed with S, in particular when produced by Powder Metallurgy (PM). The steel composition may then fulfil at least one of the following requirements:
-
Min Max N 0.01 0.04 Cu 0.5 2.1 Cr + Ni 20.5 22.0 Mo 1.2 1.6 S 0.01 Ti 0.01 Zr 0.01 Ta 0.01 Hf 0.01 Y 0.01
wherein the microstructure may fulfil at least one of the following requirements: -
- the matrix comprises ≥75 vol. % martensite,
- the matrix comprises ≤7 vol. % delta ferrite,
- the matrix comprises 2-20 vol. % austenite,
- the matrix hardness is 40-56 HRC,
- the size of all AlN particles is ≤4 μm,
- the un-notched impact toughness is ≥200 J,
- the compressive yield strength Rc0.2 is at 10-30% higher than the tensile yield strength Rp0.2.
- In a particular embodiment the steel fulfils the following requirements:
-
Min Max C 0.025 0.035 Si 0.15 0.40 Mn 0.15 0.50 Cr 11.5 12.5 Ni 8.5 10.0 Cr + Ni 20 23 Mo 1.0 2.0 Al 1.5 1.9 N 0.01 0.15 -
- wherein the microstructure fulfils at least one of the following requirements:
- the matrix comprises ≥80 vol. % martensite,
- the matrix comprises 4-20 vol. % austenite.
- wherein the microstructure fulfils at least one of the following requirements:
- The steel alloy can be provided in the form of a pre-alloyed powder having a composition as shown above.
- The pre-alloyed powder can be produced by gas atomizing. It is preferred that at least 80% of the powder particles have a size in the range of 5 to 150 μm so that the powder fulfils at least one of the following requirements:
-
Powder size distribution (in μm): 5≤ D10 ≤35 20≤ D50 ≤55 D90 ≤80 Mean sphericity, SPHT ≥0.85 Mean aspect ratio, b/l ≥0.85
wherein SPHT=4πA/P2, where A is the measured area covered by a particle projection and P is the measured perimeter/circumference of a particle projection and the sphericity (SPHT) is measured by a Camsizer in accordance with ISO 9276-6, and wherein b is the shortest width of the particle projection and 1 is the longest diameter. - It is even possible that at least 90% of the powder particles have a size in the range of 10 to 100 μm and that the powder fulfils at least one of the following requirements:
-
Powder size distribution (in μm): 10≤ D10 ≤30 25≤ D50 ≤45 D90 ≤70 Mean sphericity, SPHT ≥0.90 Mean aspect ratio, b/l ≥0.88 - The pre-alloyed described above can be used to form an article by the use of an additive manufacturing method. The article may fulfil at least one of the following requirements:
-
- the matrix comprises ≥80 vol. % martensite,
- the matrix comprises ≤5 vol. % delta ferrite,
- the matrix comprises 2-20 vol. % austenite,
- the matrix hardness is 34-56 HRC,
- the size of all AlN particles is ≤4 μm,
- the Charpy V-notch value perpendicular to the build direction is ≥5 J,
- the tensile strength Rm perpendicular to the build direction is ≥1600 MPa,
- the yield strength Rc0.2 perpendicular to the build direction is ≥1500 MPa,
- the compressive yield strength Rc0.2 perpendicular to the build direction is at least 10% higher than the tensile yield strength Rp0.2.
- Preferably, the article is at least a part of a mould for forming plastic and the said article may optionally fulfil at least one of the following requirements:
-
- the matrix comprises ≥85 vol. % martensite,
- the matrix comprises ≤2 vol. % delta ferrite,
- the matrix comprises 4-15 vol. % austenite,
- the matrix hardness is 40-50 HRC,
- the Charpy V-notch value perpendicular to the build direction is ≥10 J.
- The invention is also directed to the use of the inventive pre-alloyed powder for making a solid object by the use of any of the methods of hot isostatic pressing, powder extrusion and additive manufacturing or for providing a surface layer on a substrate by thermal spraying, laser cladding, cold spraying or overlay welding.
- The importance of the separate elements and their interaction with each other as well as the limitations of the chemical ingredients of the claimed alloy are briefly explained in the following. All percentages for the chemical composition of the steel are given in weight % (wt. %) throughout the description. The amount of hard phases is given in volume % (vol. %). Upper and lower limits of the individual elements can be freely combined within the limits set out in the claims.
- Carbon is effective for improving the strength and the hardness of the steel. However, if the content is too high, the steel may be difficult to machine after cooling from hot working. C should be present in a minimum content of 0.02%, preferably at least 0.025%. The upper limit for carbon is 0.04%, preferably 0.035%. The nominal content is 0.030%.
- Silicon is used for deoxidation. Si is also a strong ferrite former. Si is therefore limited to 0.45%. The upper limit may be 0.40, 0.35, 0.34, 0.33, 0.32, 0.31, 0.30, 0.29 or 0.28%. The lower limit may be 0.12, 0.14, 0.16, 0.18 or 0.20%. Preferred ranges are 0.15-0.40% and 0.20-0.35%.
- Manganese contributes to improving the hardenability of the steel. If the content is too low then the hardenability may be too low. At higher sulphur contents manganese prevents red brittleness in the steel. Manganese shall therefore be present in a minimum content of 0.10%, preferably at least 0.15, 0.20, 0.25 or 0.30%. The steel shall contain maximum 0.5% Mn, preferably maximum 0.45, 0.40 or 0.35%. A preferred range is 020-0.40%.
- Chromium is to be present in a content of at least 11% in order to make the steel stainless and to provide a good hardenability in larger cross sections during the heat treatment. However, high amounts of Cr may lead to the formation of high-temperature ferrite, which reduces the hot-workability. The lower limit may be 11.2, 11.4, 11.6 or 11.8%. The upper limit Cr is 13% and the amount of Cr may be limited or 12.8, 12.6, 12.4 or 12.2%. A preferred range is 11.5-12.5%.
- Nickel is an austenite stabilizer, which and suppresses the formation of delta ferrite. Nickel gives the steel a good hardenability and toughness. Nickel is also beneficial for the machinability and polishability of the steel. Nickel is essential for the precipitation hardening as it together with Al form minute intermetallic NiAl-particles during aging. However, excess Ni additions may result in too high an amount of retained austenite. The lower limit may therefore be 7.2, 7.4, 7.6, 7.8, 8.0, 8.2, 8.4, 8.6, 8.8, 9.0 or 9.1%. The upper limit may be 10.0, 9.8, 9.6 or 9.4%. A preferred range is 8.5-10 or 9.0-9.5%.
- In order to obtain an optimized strength and toughness it is desirable, that the total content of Cr and Ni is 19-23%. The lower amount may be 19.5, 20.0, 20.5 20.6, 20.7, 20.8 or 20.9%. The upper limit may be 22.8, 22.7, 22.6, 22.5, 22.4, 22.3, 22.2, 22.1, 22.0, 21.9, 21.8, 21.7, 21.6, 21.5, 21.4 or 21.3% A preferred range is 20.5-22.0%, preferably 20.5-22.0, most preferably 20.8-21.7%.
- Mo in solid solution is known to have a very favourable effect on the hardenability. Molybdenum is a strong carbide forming element and also a strong ferrite former. A controlled amount of Mo in the matrix counteracts the formation of reverted austenite during aging. For this reason the amount of Mo should be 1-2%. The lower limit may be 1.1, 1.2, 1.3 or 1.4%. The upper limit may be 1.9, 1.8, 1.7, 1.6, or 1.5%.
- Molybdenum can also be used in higher amounts in combination with Boron in order to obtain a desired amount of hard borides of the type M2M′B2, where M and M′ stand for metals. In the present case M is Mo and M′ is Fe. However, the boride may contain minor amounts of other elements such as Cr and Ni. However, in the following boride will simply be referred to as Mo2FeB2.
- The maximum content of molybdenum is therefore 25%. However, when using high Mo contents for forming borides, then the contents of Mo and B should be balanced such that the content of Mo in solid solution in the matrix remains in the range of 1-2%.
- Aluminium is used for precipitation hardening in combination with Ni. The upper limit is restricted to 2.0% in order to avoid the formation of too much delta ferrite. The upper limit may be 1.95, 1.90, 1.85, 1.80 or 1.75%. The lower limit may be 1.45, 1.50, 1.55, 1.60 or 1.65%.
- Nitrogen is a strong austenite former and also a strong nitride former. N may be used in in an amount of up to 0.75% in Nitride Dispersion Strengthened (NDS) alloys. NDS alloys can be produced with basically the same techniques as ODS alloys.
- However, for non-NDS applications the nitrogen content may be restricted to 0.15%.
- The inventors of the present invention have surprisingly found, that nitrogen can be deliberately added to the steel without impairing the polishability, provided that the size of at least 80 vol. % of AlN particles present in the matrix is limited to not more than 4 μm. Preferably, the said size may restricted to 3 μm, 2 μm or even 1 μm. The small size of the nitrides also results in a grain refining effect. The lower limit for N may then be 0.011, 0.012, 0.013, 0.014, 0.015, 0.016, 0.017, 0.018, 0.019 or 0.02%. The upper limit may be 0.14, 0.12, 1.10, 0.08, 0.06, 0.05, 0.04 or 0.03%. However, if the material is in powder form and intended for production of moulds or dies by the use of AM, then it is to be considered that a too high nitrogen content may result in too high an amount of retained austenite. Accordingly, for applications where the amount of austenite in structure is to be limited, then the upper limit of nitrogen can be set to 0.040, 0.035, 0.030, 0.025 or 0.020%.
- Cu is an optional element, which may contribute to increase the hardness and the corrosion resistance of the steel. The ε-Cu phase formed during aging not only reinforces the steel by precipitation hardening, but also affects the precipitation kinetics of the intermetallic phases. In addition thereto, it would appear that additions of Cu result in a slower growth of the intermetallic phase (NiAl) at higher working temperatures. The upper limit for Cu may be 2.3, 2.1, 1.9, 1.7, 1.5, 1.3, 1.1, 0.9, 0.7, 0.5, 0.3 or even 0.2%. The lower limit for Cu may 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 or 0.9%.
- However, it is not possible to extract copper from the steel once it has been added. This makes the scrap handling more difficult. For this reason, copper is an optional element and needs not be added. The maximum allowable impurity content can be 0.2, 0.15 or 0.10%.
- Boron is an optional element that can be used in small amounts in order to increase the hardenability and to improve the hot workability of the stainless steel. The upper limit may then be set to 0.007, 0.006, 0.005 or 0.004%.
- Boron can also be used in higher amounts as a hard phase-forming element. B should then be at least 0.2% so as to provide the minimum amount of 3% hard phase Mo2FeB2. The amount of B is limited to 2.0% for not making the alloy too brittle. The lower limit may be set to 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 or 1.5%. The upper limit may be set to 1.4, 1.5, 1.6, 1.7, 1.8 or 1.9%.
- S may optionally be added in order to improve the machinability of the steel. If S is used for this purpose, then S is deliberately added to the steel in an amount of 0.01-0.25%. At higher sulphur contents there is a risk for red brittleness. Moreover, high sulphur contents may have a negative effect on the fatigue properties and on the polishability of the steel. The upper limit shall therefore be 0.25%, preferably 0.1% most preferably 0.03%. A preferred range is 0.015-0.030%. However, if not deliberately added, then the amount of S is restricted to impurity contents as set out below.
- Nb is a strong carbide and nitride former. The content of this elements should therefore be limited in order to avoid the formation of undesired carbides and nitrides. The maximum amount of Nb is therefore 0.01%. Nb is preferably limited to 0.005%.
- These elements may form compounds with C, B, N and/or O. They can be used to produce an Oxide Dispersion Strengthened (ODS) or a Nitride Dispersion Strengthened (NDS) alloy. The upper limit is then 2% for each of these elements. The upper limit may be 1.5, 1.0, 0.5 or 0.3%. However, if these elements are not deliberately added for making an ODS alloy, then the upper limit may be 0.1, 0.05, 0.01 or 0.005%.
- These elements may optionally be added to the steel in the claimed amounts for different reasons. These elements are commonly used to modify the non-metallic inclusion and/or in order to further improve the machinability, hot workability and/or weldability of the steel. The oxygen content is then preferably limited to 0.03%. However, if Oxygen is used in order to form an Oxide Dispersion Strengthened (ODS) alloy, then the upper limit may be as high as 0.80%. The oxide can be admixed to a powder of be formed in-situ, e.g. by gas atomizing, in particular by using Gas Atomizing Reaction Synthesis (GARS) or during an Additive Manufacturing (AM) method, in particular through atmospheric reaction in Liquid Metal Deposition (LMD).
- P, S and O are the main impurities, which may have a negative effect on the mechanical properties of the steel. P may therefore be limited to 0.05, 0.04, 0.03 0.02 or 0.01%. If sulphur is not deliberately added, then the impurity content of S may be limited to 0.05, 0.04, 0.003, 0.001, 0.0008, 0.0005 or even 0.0001%.
- The alloys of the present invention can be produced by any suitable method. Non-limiting examples of suitable methods include:
-
- a) Conventional melt metallurgy followed by casting and hot working.
- b) Powder Metallurgy (PM).
- PM powders can be produced by conventional gas- or water-atomization of pre-alloyed steel. The powders can be used for thermal spraying, overlay welding, additive manufacturing (AM) or Metal Injection Moulding (MIM).
- However, if the powder shall be used for AM, then gas-atomization is the preferred atomization method, because it is important to use a technique, that produces powder particles having a high degree of roundness and a low amount of satellites. In particular, the close-coupled gas atomization method can be used for this purpose.
- Powders produced by PM can be consolidated by Hot Isostatic Pressing (HIP) and/or by extrusion. The materials can be used as compacted or after subsequent hot working.
- The maximum size of the powder particles should normally be limited to 500 μm and, depending on the intended use, specific powder fractions may be used. For AM the maximum size range is 5-150 μm, and the preferred size range is 10-100 μm with a mean size of about 25-45 μm. For MIM the preferred maximum size is 50 μm, for thermal spraying preferred ranges is 32-125 μm and 20-90 μm and for overlay welding the preferred range is 45-250 μm.
- The AM methods of prime interest are Liquid Metal Deposition (LMD), Selective Laser Melting (SLM) and Electron Beam (EB) melting. The powder characteristics are also of importance for AM. The powder size distribution measured with a Camsizer according to ISO 4497 should fulfil the following requirements (in μm):
-
5≤D10≤35 -
20≤D50≤55 -
D90≤80 - Preferably, the powder should fulfil the following size requirements (in μm):
-
10≤D10≤30 -
25≤D50≤45 -
D90≤70 - Even more preferred is that the coarse size fraction D90 is limited to ≤60 μm or even ≤55 μm.
- The sphericity of the powder should be high. The sphericity (SPHT) can be measured by a Camsizer and is defined in ISO 9276-6. SPHT=4πA/P2, where A is the measured area covered by a particle projection and P is the measured perimeter/circumference of a particle projection. The mean SPHT should be at least 0.80 and can preferably be at least 0.85, 0.90, 0.91, 0.92 0.93, 0.94 or even 0.95. In addition, not more than 5% of the particles should have a SPHT≤0.70. Preferably said value should be less than 0.70, 0.65, 0.55 or even 0.50. In addition to SPHT, the aspect ratio can be used in the classifying of the powder particles. The aspect ratio is defined as b/1, wherein b is the shortest width of the particle projection and 1 is the longest diameter. The mean aspect ratio should preferably be at least 0.85 or more preferably 0.86, 0.87, 0.88, 0.89, or 0.90.
- The inventive alloy is a precipitation hardenable steel having a martensitic matrix, which may comprise other microstructural constituents such as delta ferrite and austenite. The austenite may comprise retained and/or reverted austenite.
- The inventive alloy can be hardened by aging in the temperature range of 425-600° C. to a desired hardness in the range of about 34-56 HRC.
- The amount of delta ferrite should preferably be restricted to ≤7 vol. %, preferably ≤5 vol. %, more preferably ≤3 vol. % for not impairing the hot workability.
- The austenite consists of retained and/or reverted austenite, in the following, austenite. Pre-alloyed powder produced by atomizing may contain substantial amounts of austenite but the amount of austenite in finished parts may be reduced to a lower level by solution heat treatment and/or ageing, if there is a fear that the austenite content is so high that it could lead to problems e.g. with respect to dimensional stability. The amount of austenite in the microstructure may therefore be limited to 22, 20, 18, 16, 14, 12, 10, 8, 6, 4 or 2 vol. %. However, austenite has a positive effect on the mechanical properties of the material, in particular the toughness, and is therefore a desired microstructural constituent in many applications.
- The inventive alloy can be hardened by aging in the temperature range of 425-600° C. to a desired hardness in the range of about 34-56 HRC.
- An alloy was produced in conventional way by induction melting, casting and forging. The alloy had the composition (in wt. %): C: 0.03, Si: 0.3, Mn: 0.2, Cr: 12.0, Ni: 9.3, Mo: 1.4, Al: 1.7, N: 0.017, balance Fe and impurities. The inventive alloy was compared to a commercial available steel of the type steel PH 13-8Mo (Böhler N709). The comparative alloy had the following nominal composition (in wt. %): C: 0.03, Si: ≤0.08, Mn: ≤0.08, Cr: 12.7, Ni: 8.1, Mo: 2.2, Al: 1.1, balance Fe.
- The inventive alloy differs from the comparative steel mainly in higher amounts of Mn, Si, Al and N and lower amounts of Mo dissolved in the matrix.
- The inventive steel and the comparative steel were both hardened to 50 HRC and subjected to un-notched impact testing using a standard specimen size of 10 mm×10 mm×55 mm. The inventive alloy was found to have an un-notched impact strength of 255 J, whereas the impact strength of the known steel was only 120 J.
- The reason for this difference is presently not fully understood. However, it would appear that small differences in the matrix composition lead to differences in the precipitation kinetics such that the type and distribution of the precipitates are different. The lower content of Mo may also result in a reduced risk of the formation of reverted austenite during the heat treatment and thereby also a reduced risk for the precipitation of Mo- and Cr-rich carbides. The addition of Al may result in a grain refinement that is beneficial for the toughness. Hence, it would appear plausible that one or more of these factors in combination result in an improved toughness of the inventive steel.
- A base alloy having the composition similar to the alloy of Example 1 was produced in conventional way by induction melting, casting and forging. A ESR-remelted bar of the alloy was subjected to vacuum induction melting and closed couple gas atomization processing in order to obtain a powder suitable for AM processing. The gas to metal weight ratio during the atomization was 3:1. In order to avoid oxygen contamination, high purity (6N) nitrogen gas was used for the atomization. The particles obtained were examined with respect to size and shape by dynamic image processing according to ISO 13322-2. The powder was sieved in order to remove particles larger than 50 μm and smaller than 20 μm. The sieved powder was found to have the following size distribution: D10: 23 μm, D50: 34 μm and D90: 49 μm. The mean sphericity was 0.95 and the mean aspect ratio was 0.93. The powder had an oxygen content of 0.021% and a nitrogen content of 0.013%. The morphology of this powder was examined by Scanning Electron Microscopy (SEM and the powder was found to be almost fully spherical with a very low amount of satellites.
- The Apparent Density (AD) was 4.3 g/cm3 and the Tap Density (TD) was 5.2 4.3 g/cm3.
- Accordingly, the powder produced would be expected to be suitable for AM processing.
- The suitability of this powder for AM was tested by building a part by SLM in an EOS M290 system using the following processing parameters: Layer thickness 30 μm, laser power 170 W, scan speed 1250 mm/s, hatch distance 0.10 mm. The hatch mode was stripes.
- The as-built samples thus obtained had a density of 99.4% of the theoretical density (TD) and a hardness of 35 HRC at room temperature. The amount of austenite was about 23% in the sample. An examination in SEM using EBSD revealed that the austenite phase was extremely fine in size and dispersed at the boundaries of the martensite blocks.
- The influence of the thermal treatment of the built sample was examined. After ageing at 525° C. for 4 h the amount of austenite was reduced to 16 vol. %. However, an intermediate solution treatment at 850° C. for 30 minutes reduced the amount of austenite to 4 vol. %. The hardness of the solution annealed and aged sample was 50 HRC.
- Hence, the solution annealed and the aged sample have the same hardness as the conventionally produced sample of Example 1. The reason for this might be, that the conventionally produced sample also has an austenite content of about vol. 4%. It was therefore decided to compare the mechanical properties of the solution treated and aged AM sample with the properties of the conventionally produced steel in Example 1. The strength and elongation values were measured by uniaxial tensile testing and the impact toughness was measured by the Charpy V-notch test. The results are given below in Table 1. It can be seen that the material produced by AM has a considerably higher Impact toughness than the conventionally produced material and that the other mechanical values are comparable.
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TABLE 1 Results of the mechanical testing. Rm Rp02 Elongation A5 Impact toughness Sample (MPa) (MPa) (%) (J) Conv. (EX. 1) 1700 1600 10 3 (S-T) 6 (L-T) AM (EX. 3). 1700 1640 9 19 Perpendicular to build plate AM (EX. 3) 1650 1560 10 22 Parallel to build plate - The corrosion and wear testing revealed, that the two materials are equally good. The polishability was also examined and it was found that the AM material exhibits an excellent polishability. It was possible to achieve a comparably good high quality gloss surface for both materials, although the oxygen content was about 10 times higher for the AM material. However, surprisingly it was found that the AM material was much easier to polish in that the AM-material could be polished to the same gloss with fewer steps in a shorter time.
- The steel of the present invention is useful in large moulds or dies requiring a good corrosion resistance and a uniform hardness. The steel of the present invention is particular for making articles by AM.
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2017
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- 2017-06-07 RU RU2019100694A patent/RU2744788C2/en active
- 2017-06-07 US US16/310,185 patent/US20190368016A1/en not_active Abandoned
- 2017-06-07 ES ES17813692T patent/ES2775755T3/en active Active
- 2017-06-07 WO PCT/SE2017/050604 patent/WO2017217913A1/en unknown
- 2017-06-07 CN CN201780036780.7A patent/CN109312439B/en active Active
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2022
- 2022-06-14 JP JP2022095971A patent/JP2022133306A/en not_active Withdrawn
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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US20190055633A1 (en) * | 2017-08-16 | 2019-02-21 | U.S. Army Research Laboratory Attn: Rdrl-Loc-I | Methods and compositions for improved low alloy high nitrogen steels |
EP3912816A1 (en) * | 2020-05-18 | 2021-11-24 | Daido Steel Co., Ltd. | Metal powder |
CN113751703A (en) * | 2020-05-18 | 2021-12-07 | 大同特殊钢株式会社 | Metal powder |
US11807921B2 (en) | 2020-05-18 | 2023-11-07 | Daido Steel Co., Ltd. | Metal powder |
CN113737081A (en) * | 2021-08-31 | 2021-12-03 | 中国科学院上海应用物理研究所 | Stainless steel smelting method, stainless steel modification method and stainless steel |
EP4180549A1 (en) * | 2021-11-10 | 2023-05-17 | Daido Steel Co., Ltd. | Fe-based alloy for melt-solidification-shaping and metal powder |
CN114507817A (en) * | 2022-01-20 | 2022-05-17 | 上海材料研究所 | Ultra-low carbon cobalt-free high-strength corrosion-resistant alloy and preparation method and application thereof |
CN116275011A (en) * | 2023-05-19 | 2023-06-23 | 清华大学 | Powder for additive manufacturing, ultra-high strength and toughness steel, and preparation method and application thereof |
Also Published As
Publication number | Publication date |
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WO2017217913A1 (en) | 2017-12-21 |
EP3472365A1 (en) | 2019-04-24 |
KR20190046768A (en) | 2019-05-07 |
BR112018075617A2 (en) | 2019-04-09 |
SE539763C2 (en) | 2017-11-21 |
CN109312439B (en) | 2020-11-27 |
ES2775755T3 (en) | 2020-07-28 |
JP7160689B2 (en) | 2022-10-25 |
KR102436457B1 (en) | 2022-08-24 |
BR112018075617B1 (en) | 2022-06-14 |
RU2744788C2 (en) | 2021-03-15 |
TW201809315A (en) | 2018-03-16 |
SE1650850A1 (en) | 2017-11-21 |
CN109312439A (en) | 2019-02-05 |
MX2018015012A (en) | 2019-04-11 |
EP3472365A4 (en) | 2019-05-15 |
JP2019523821A (en) | 2019-08-29 |
JP2022133306A (en) | 2022-09-13 |
RU2019100694A (en) | 2020-07-16 |
CA3027852A1 (en) | 2017-12-21 |
RU2019100694A3 (en) | 2020-08-18 |
EP3472365B1 (en) | 2019-11-27 |
TWI715776B (en) | 2021-01-11 |
US20230035760A1 (en) | 2023-02-02 |
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